毛发、尿液中依托咪酯及代谢物HPLC-MS/MS检测  

Determination of Etomidate and Its Metabolite in Hair and Urine by HPLC-MS/MS

作　　者：吴永富 王燕军[2] 代勇[3] 张鑫 周奎霖 蔡玉刚 WU Yongfu;WANG Yanjun;DAI Yong;ZHANG Xin;ZHOU Kuilin;CAI Yugang(Institute of Forensic Science of Luzhou Public Security Bureau,Luzhou 646000,Sichuan,China;Criminal Investigation Bureau,Sichuan Provincial Public Security Department,Chengdu 610015,China;Sichuan Police College,Luzhou 646000,Sichuan,China;Chengdu Insight Medical Laboratory Co.LTD,Chengdu 610041,China)

机构地区：[1]泸州市公安局刑事科学技术研究所,四川泸州646000 [2]四川省公安厅刑事侦查局,成都610015 [3]四川警察学院,四川泸州646000 [4]成都英视医学检验实验室有限公司,成都610041

出　　处：《刑事技术》2025年第1期61-67,共7页Forensic Science and Technology

基　　金：2022年四川省警察学院研究生创新项目(22YCX046)。

摘　　要：本文建立高效液相色谱-三重四极杆串联质谱仪(HPLC-MS/MS)检测毛发和尿液中依托咪酯及其代谢物依托咪酯酸的检测方法。毛发样品经研磨粉碎后,经甲醇超声提取,尿液样品经乙腈沉淀蛋白高速离心过0.22μm滤膜后,采用Agilent Eclipse Plus C18 RRHD(3.0 mm×150 mm×1.8μm)色谱柱,以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,流速0.5 mL/min;选择电喷雾离子源,多反应监测(MRM)正离子模式进行监测。实验表明,尿液中依托咪酯和依托咪酯酸在0.5~50 ng/mL的浓度范围,毛发中依托咪酯和依托咪酯酸在0.025~2.5 ng/mg浓度范围内线性关系良好,R^(2)值均大于0.9925,提取回收率为91.0%~107.5%,日内和日间精密度RSD为0.4%~7.4%,日内和日间准确度为91.5%~110.8%。对实际案例中的6份毛发和4份尿液样本进行检测,检测结果表明,6份毛发均检出依托咪酯原体,其中2份毛发检出代谢物依托咪酯酸且含量远低于原体;4份尿液中2份检出依托咪酯和代谢物依托咪酯酸且代谢物含量远高于原体。本文建立的方法能快速对吸食依托咪酯人员的毛发和尿液中依托咪酯及代谢物进行定性定量分析。A method was developed for the determination of etomidate and its metabolite etomidate acid in hair and urine by high performance liquid chromatography-triple quadrupole tandem mass spectrometer(HPLC-MS/MS).The hair samples were ground and extracted by ultrasonic extraction with methanol.After protein was precipitated by acetonitrile,the urine samples were centrifuged at high speed and passed through 0.22μm filter membrane,and then Agilent Eclipse Plus C18 RRHD(3.0 mm×150 mm×1.8μm)column was used for analysis.Gradient elution was performed with 0.1%formic acid aqueous solution-acetonitrile as mobile phase at theflow rate of 0.5 mL/min.Electrospray ion source and multiple reaction monitoring(MRM)positive ion mode were selected.The results showed that the linear relationship of the two compounds exhibited good linearity in the concentration range of 0.5 to 50 ng/mL in urine and 0.025 to 2.5 ng/mg in hair,and the R^(2) value was greater than 0.9925.The extraction recoveries ranged from 91.0%to 107.5%,and the intra-day and inter-day precision RSD was 0.4%to 7.4%,while the intra-day and inter-day accuracy was 91.5%to 110.8%.In the actual cases,six hair samples and 4 urine samples were tested,and the test results showed that etomidate was detected in all six hair samples,and the metabolite etomidate acid was detected in two hair samples,but the concentration was much lower than the original.Etomidate and metabolite etomidate acid were detected in two urine samples,and the metabolite concentration was much higher than the original.In conclusion,this method can be used for rapid qualitative and quantitative analysis of etomidate and its metabolite in the hair and urine of etomidate users.

关 键 词：依托咪酯 依托咪酯酸 高效液相色谱-三重四级杆串联质谱仪(HPLC-MS/MS) 毛发 尿液 

分 类 号：DF795.1[医药卫生—法医学]